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A kind of preparation method of cefepime hydrochloride

A technology of cefepime hydrochloride and aminocephalosporanic acid, which is applied in the field of preparation of pharmaceutical compounds, can solve the problems of expensive raw materials, unsuitability for large-scale industrial production, and low yield, and achieve simple operation, improved industrial hygiene environment, and improved conversion rate effect

Inactive Publication Date: 2011-12-14
HARBIN PHARMA GRP CO LTD GENERAL PHARMA FACTORY
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Problems solved by technology

[0018] Some of the above methods use expensive raw materials, some are not suitable for industrialized large-scale production, and some yields are relatively low. In order to solve the problems in industrialized production, the present invention provides a new preparation method of cefepime hydrochloride

Method used

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  • A kind of preparation method of cefepime hydrochloride

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Embodiment 1

[0035] 1. Dissolve 100g of 7-aminocephalosporanic acid (7-ACA) in 500g of dichloromethane solvent (wet the 7-ACA with dichloromethane before feeding and then use the wet feeding method), add 100g of N, O-bistrimethylsilane Acetamide (BSA), stirred at room temperature for two hours, cooled to 10°C, added 80g N, N-diethylaniline, 120g iodotrimethylsilane, and reacted for 3-4 hours. When 7ACA<1.0g / l is detected by liquid phase, the reaction can be regarded as complete.

[0036] 2. At the end of the reaction, add 50g of N-methylpyrrolidine dropwise. After the dropwise addition, keep the reaction at 0-5°C for 1 hour. If the iodide residue is less than 1.0%, the reaction can be ended.

[0037] 3. Add the above solution to 30g of methanol, stir and react for 1 hour, then add a hydrochloric acid solution of 210g of concentrated hydrochloric acid and 210g of water, the temperature of the feed liquid during the dropwise addition should not exceed 10°C, stir quickly until it is completel...

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Abstract

The invention relates to a preparation of a pharmaceutical compound, in particular to a preparation method of cefepime hydrochloride. The present invention is an improvement after overcoming the shortcomings of the commonly used industrial production process and laboratory process. The improvement is that: 7-ACA adopts wet feeding when feeding; when 7-ACA is protecting, the protection used BSA is used as the agent; in the crystallization process of 7-MPCA, the process of adding crystallization solvent and growing crystals at room temperature is added; the amount of activated carbon used in the decolorization of cefepime hydrochloride is reduced.

Description

Technical field: [0001] The invention relates to the preparation of a pharmaceutical compound, in particular to a preparation method of cefepime hydrochloride. Background technique: [0002] Cefepime is a broad-spectrum fourth-generation cephalosporin. [0003] Its English name: Cefepime hydrochloride [0004] CAS number: 123171-59-5, [0005] Chemical name: (6R, 7R)-7-[(Z)-2-(2-amino-4-thiazolyl)-2-methoxyimine]acetamido-3-[1-(1-methyl Pyrrolidinyl)methyl]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylate hydrochloride monohydrate [0006] Molecular formula: C19H25ClN6O5S2.HCl.H2O [0007] [0008] Cefepime achieves its bactericidal effect by inhibiting the biosynthesis of bacterial cell walls. In vitro tests have shown that this product has effects on both Gram-positive and Gram-negative bacteria. This product has a low affinity to the β-lactamase encoded by the bacterial chromosome, can be highly resistant to the hydrolysis of most β-lactamases, and can qui...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/46C07D501/04
Inventor 吴志军赵玉新王喜军李秀艳梁轶群李国峰王亚玲李志伟
Owner HARBIN PHARMA GRP CO LTD GENERAL PHARMA FACTORY
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